GC法测定水产品中的甲基汞残留

Determination of Methylmercury in the Aquatic Product by Gas Chromatography

采用气相色谱(GC)法测定水产品中的甲基汞残留。样品前处理方法在HZ-HJ-SZ-0097(《环境甲基汞的测定气色谱法》)所规定的基础上,增加萃取溶剂体积;色谱条件优化如下:毛细管色谱柱Supelcowax-10(30m×0.53mm×0.5μm),柱温为210℃,进样口温度为210℃,ECD检测器温度为300℃,尾吹(N2)50mL/min,流速为7.0mL/min,不分流进样。测定结果表明,甲基汞的峰形尖锐,响应灵敏度高,标准的线性相关系数为0.9992,加标样品测定的相对标准偏差(RSD)为2.1%(n=6),最小检出限为0.1μg/kg,回收率均为85%～92%。测定结果显示,该方法具有快速、灵敏、可靠、简便、重现性好等特点。

Gas chromatograph was used to detect methylmercury in the aquatic product. The method for sample pretreatment followed the industry standard HZ-HJ-SZ-0097 （Environment, Determination of Methylmecury, and GC）, but the extraction solvent volume was increased; chromatography conditions were optimized： capillary chromatogram column （Supelco wax-10）, column temperature 210℃; injector temperature： 210℃; ECD temperature： 280℃; auxiliary gas （N2）： 50ml/min; gas flow rate： 7.0 m l/min; inject mode： splitless. The detection result showed that the methylmercury had a sharp peak and sensitive response. The correlation modulus of linearity was 0.999 2, and the relative standard deviations of the sample was 2.1% （n= 6）. The minimum detection of Sudan dyes was 0.1 μg/kg. The average recovery of methylmercury was 85-92%. All these indicated that this method is rapid, sensitive, simple, accurate and reproducible.